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液相色谱-串联质谱法测定血清和尿液中硝基咪唑类药物残留

Residue Determination of Nitroimidazoles in Sera and Urine by High Performance Liquid Chromatography-tandem Mass Spectrometry

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【作者】 张金玲郭礼强孙军吴翠玲

【Author】 ZHANG Jin-ling;GUO Li-qiang;SUN Jun;WU Cui-ling;Weifang Entry-Exit Inspection and Quarantine Bureau;Agilent Technologies Co.LTD in China;

【机构】 潍坊出入境检验检疫局安捷伦科技(中国)有限公司

【摘要】 为建立血清和尿液中甲硝唑、羟基甲硝唑、二甲硝咪唑和羟基二甲硝咪唑的高效液相色谱-串联质谱(HPLC-MS/MS)快速测定方法,样品用乙酸乙酯提取,经PCX固相萃取柱净化,Eclipse Plus C18色谱柱(3.0mm×100mm,1.8μm)分离,进行HPLC-MS/MS分析。结果表明,甲硝唑、羟基甲硝唑、二甲硝咪唑及羟基二甲硝咪唑在0.20μg/L~50μg/L范围呈良好线性,线性相关系数均大于0.995,检出限为0.20μg/L,定量下限为0.50μg/L。样品在定量下限1、2、10倍3个加标水平下的平均回收率为89.3%~108.2%,相对标准偏差(RSD)为2.63%~10.0%。该方法灵敏、简便、准确,可用于血清和尿液中硝基咪唑类药物的检测分析。

【Abstract】 A method for the determination of metronidazole,hydroxy metronidazole,dimetridazole and hydroxy dimetridazole in sera and urine by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established.The target compounds were purified with solid phase extraction column of PCX after extraction by ethyl acetate.Then the samples was separated by an Eclipse Plus C18 column(3.0mm×100mm,1.8μm)and analyzed by HPLC-MS/MS.The calibration curves were linear in the range of 0.2μg/L-50μg/L for metronidazole,hydeoxy metronidazole,dimetridazole and hydeoxy dimetridazole with correlation coefficient(r)more than 0.995.The LOD was 0.2μg/L and the LOQ was 0.5μg/L.The average recoveries(n=6) in feed samples at three spiked levels(1 times,2 times,10 times)ranged from 89.3%-108.2% with relative standard deviations(RSDs) of 2.63%-10.0%.The method was sensitive,convenient and accurate,and could satisfy the demand of detection and analysis of nitroimidazoles in serum and urine samples.

【基金】 山东出入境检验检疫局科研基金项目(SK201349);潍坊市2015年科学技术发展计划项目(2015ZJ1101)
  • 【文献出处】 动物医学进展 ,Progress in Veterinary Medicine , 编辑部邮箱 ,2017年07期
  • 【分类号】O657.63;R96
  • 【被引频次】6
  • 【下载频次】133
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